Dimethylformamide dimethyl acetal → HCID 13039371, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of 130 g (40.0 mmol) of 1-(2,6-dimethylphenylcarbamoyl)-3-(2,2,2-trifluoroethyl) guanidine hydrochloride in CH3CN (50 ml) were added 95 g (80.0 mmol) of DMF-DMA and the mixture heated at reflux for two hours. The solvent was removed under vacuum, and the residue partitioned between CHCl3 and H2O. The layers were separated and the aqueous layer was extracted with CHCl3 (1×100 ml). The extracts were dried (MgSO4) and concentrated to give a white solid which was crystallized from absolute EtOH to give after heating under vacuum at 100° C. for one hour; 9.5 g (80%) of 1-(2,6-dimethylphenyl)-4-(2,2,2-trifluoroethylamino)dihydro-1,3,5-triazin-2-one; melting point 212°-3° C.

Provenance & Evidence